摘要：本文建立了腐竹中测定乌洛托品的方法，以乙腈提取腐竹中乌洛托品，加盐酸水解生成甲醛，以3-甲基-2-苯并噻唑啉酮腙盐酸盐水合物（酚试剂）和硫酸高铁铵与甲醛反应生成蓝绿色化合物，通过在630 nm测吸光度来间接测定乌洛托品。实验考察了盐酸的用量、水解温度、吸附剂种类、反应时间等实验条件的影响。用乙腈溶液超声10 min提取腐竹中的乌洛托品，用1.5 g中性氧化铝吸附溶液中的悬浊物，在50 ℃和0.5 ml盐酸分解得到的实验结果最佳。实验显示：脂肪、糖、蛋白质、苯丙氨酸、等对实验结果没有干扰，亚硫酸盐对实验稍有干扰。本实验线性范围在0.6～6.0 μg/ml 的范围内线性关系良好，相关系数 R2=0.9933。腐竹中的加标回收率平均88.2%。其检出限低，准确性高，稳定性好，可用于腐竹中乌洛托品的检测，相对标准偏差为1.72%。7801
关键词： 乌洛托品；腐竹；中性氧化铝；酚试剂
Determation of hexamethylenetetramine in the Fuzhu by spectrophotometry
Abstact: The thesis presents a spectrophotometric method for determing hexamethylenetetramine in fuzhu. The sample was extracted by acetonitrile. Hexamethylenetetramine is hydrolyzed into formaldehyde by hydrochloric acid. The formaldehyde can be reacted with 3-methyl-2-benzothiazolinone ketone hydrazone hydrochloride (Sawicki's Reagent) and ferric ammonium sulfate to form a blue-green compound, which can be measured by spectrophotometry at 630 nm. Some experimental conditions were investigated like the amount of hydrochloric acid, hydrolysis temperature, adsorbent, reaction time and so on. The result shows that the fat, sugar, protein, phenylalanine, did not interfere with the determination. Sulfite had some interfere. According to above experiment, 1.5 g neutral alumina was used to adsorb opaque solution, and 0.5 ml hydrochloric acid at 50 ℃ was used to hydrolyze hexamethylenetetramine. The method showed a good linearity at the range of 0.6～6.0 μg/ml for urotropine with R2=0.9933. The recoveries average 88.2%. The method was low detection limit, high accuracy, good stability which can be used for the detection of hexamethylenetetramine in fuzhu .
KeyWords: Hexamethylenetetramine；fuzhu； neutral alumina；Sawicki's Reagent
目录
1 前言 1
1.1选题意义 1
2文献综述 2
2.1乌洛托品理化性质 2
2.2乌洛托品用途 2
2.3乌洛托品检测方法 2
2.3.1 甲醛检测法 3
2.3.1.1 光度法 3
2.3.1.2 催化动力学法 4
2.3.1.3 化学发光法 4
2.3.1.4高效液相色谱法 4
2.3.2 氨检测法 5
2.3.2.1 光度法 5
2.3.2.2 凯氏蒸馏定氮法 5
2.3.2.3 酸碱滴定法(药典) 5
2.3.2.4 氰选择性电极法 6
2.3.3 直接测乌洛托品法 6
2.4文献讨论 8
3实验部分 10
3.1仪器与试剂 10
3.1.1仪器 10
3.1.2试剂 10
3.1.3实验药品 10
3.2样品测定方法 11
3.3乌洛托品分析方法研究 11
3.3.1乌洛托品分解条件考察-温度、盐酸用量、时间 11
3.3.2乌洛托品的标准曲线 11
3.3.3乌洛托品的显色的重复性 11
3.3.4乌洛托品分解显色时间 11
3.4腐竹样品分析条件的考察 12
3.4.1腐竹中乌洛托品提取和分解 12 腐竹中乌洛托品的测定方法研究+文献综述:http://www.751com.cn/shiping/lunwen_5884.html